Glass Ionomer Cements with Improved Bioactive and Antibacterial Properties

64 Pages·2016·2.14 MB·English

Digital Comprehensive Summaries of Uppsala Dissertations
from the Faculty of Science and Technology 1413
Glass Ionomer Cements
with Improved Bioactive and
Antibacterial Properties
SONG CHEN
ACTA
UNIVERSITATIS
ISSN 1651-6214
UPSALIENSIS
ISBN 978-91-554-9670-8
UPPSALA
urn:nbn:se:uu:diva-301924
2016
Dissertation presented at Uppsala University to be publicly examined in Å2005,
Ångströmlaboratoriet, Lägerhyddsvägen 1, Uppsala, Friday, 14 October 2016 at 09:15 for
the degree of Doctor of Philosophy. The examination will be conducted in English. Faculty
examiner: Associate Professor Jie Zhou (Delft University of Technology).
Abstract
Chen, S. 2016. Glass Ionomer Cements with Improved Bioactive and Antibacterial Properties.
Digital Comprehensive Summaries of Uppsala Dissertations from the Faculty of Science and
Technology 1413. 62 pp. Uppsala: Acta Universitatis Upsaliensis. ISBN 978-91-554-9670-8.
Dental restorative cements are placed in a harsh oral environment where they are subjected
to thermal shock, chemical degradation, and repeating masticatory force. The ideal restorative
dental cements should have superior mechanical properties, chemical stability, aesthetic, good
handling properties, biocompatibility, antibacterial properties, and preferably bioactivity. This
thesis presents research on dental restorative cements with enhanced properties. The overall aim
was to increase the bioactivity and antibacterial properties of dental restorative cements without
affecting their other properties.
The effect from adding calcium silicate to glass ionomer cement (GIC) was investigated. The
results showed that calcium silicate could increase the bioactivity and reduce the cytotoxicity of
conventional glass ionomer cement without compromising its setting and mechanical properties.
Hydroxyapatite (HA) with a high aspect ratio and thin nacreous-layered monetite sheets were
also synthesized. Nano HA particles with an aspect ratio of 50 can be synthesized by both
precipitation and hydrothermal methods. The aspect ratio was controlled via the pH of reaction
medium. Thin nacreous-layered monetite sheets were synthesized through a self-assembly
process in the presence of an amine based cationic quaternary surfactant. Temperature, pH, and
presence of surfactant played essential roles in forming the nacreous-layered monetite sheets.
Then the effect from adding silver doped HA and monetite particles was investigated. The results
showed that the antibacterial properties of GIC could be increased by incorporating silver doped
HA and monetite particles. Further examination showed that the pH change, F- ion release,
and concentration of released Ag+ ions were not responsible for the improved antibacterial
properties.
The quasi-static strengths and compressive fatigue limits of four types of the most
commonly used dental restorations were evaluated. In our study, resin modified GIC and resin-
based composite showed superior static compressive strength and fatigue limits compared to
conventional GIC. The static compressive strength of dental cements increased with the aging
time. However, aging had no effect on the compressive fatigue limit of resin modified GIC
and resin-based composite. The compressive fatigue limit of conventional GIC even showed a
drastic decrease after aging.
Keywords: biomaterial, glass ionomer cement, bioactivity, hydroxyapatite, monetite, calcium
silicate
Song Chen, Department of Engineering Sciences, Applied Materials Sciences, Box 534,
Uppsala University, SE-75121 Uppsala, Sweden.
© Song Chen 2016
ISSN 1651-6214
ISBN 978-91-554-9670-8
urn:nbn:se:uu:diva-301924 (http://urn.kb.se/resolve?urn=urn:nbn:se:uu:diva-301924)
To my family

List of Papers
This thesis is based on the following papers, which are referred to in the text
by their Roman numerals.

I Chen, S., Cai, Y., Engqvist, H., Xia, W. (2016) Enhanced bio-
activity of glass ionomer cement by incorporating calcium sil-
icates. Biomatter, 6(1):e1123842-1 - e1123842-13
II Chen, S. Mestres, G. Lan, W., Xia, W., Engqvist, H. (2016)
Cytotoxicity of modified glass ionomer cement on odontoblast
cells. Journal of Materials Science: Materials in Medicine
27(7):116
III Chen, S., Öhman, C., Jefferies, S.R., Holy, G., Xia, W.,
Engqvist H. (2016) Compressive fatigue limit of four types of
dental restorative materials. Journal of the Mechanical Behav-
ior of Biomedical Materials, 61:283-289
IV Chen, S., Pujari-Palmer, S., Rubino, S., Westlund, V., Ott, M.,
Engqvist, H., Xia, W. (2015) Highly repeatable synthesis of
nHA with high aspect ratio. Materials Letters, 159:163-167
V Chen, S., Grandfield, K., Yu, S., Engqvist, H., Xia, W. (2016)
Synthesis of calcium phosphate crystals with thin nacreous
structure. CrystEngComm, 18(6):1064-1069
VI Chen, S., Gururaj, S., Xia, W., Engqvist, H. Synthesis of Ag
doped calcium phosphate particles and their antibacterial ef-
fect as additives in dental glass ionomer cements. Accepted by
Journal of Materials Science: Materials in Medicine
Reprints were made with permission from the respective publishers.
Author’s Contributions
Paper I: Major part of planning, experiment work and writing
Paper II: Part of planning and experiment work, major part of writing
Paper III: Major part of planning, experiment work and writing
Paper IV: Major part of planning, experiment work and writing
Paper V: Major part of planning, experiment work and writing
Paper VI: Major part of planning, experiment work and writing
Also published
 Cai, Y., Chen, S., Grandfield, K., Engqvist, H., Xia, W. (2015)
Fabrication of translucent nanoceramics via a simple filtration
method. RSC Advances, 5(121):99848-99855.

 Pujari-Palmer, S., Chen, S., Rubino, S., Weng, H., Xia, W.,
Engqvist, H., Tang, L., Ott, M. (2016) In vivo and in vitro
evaluation of hydroxyapatite nanoparticle morphology on the
acute inflammatory response. Biomaterials, 90:1-11.

Contents
Introduction ................................................................................................... 13 
Aims and objectives ...................................................................................... 15 
Dental restorative materials .......................................................................... 16 
Glass ionomer cements (GICs) ..................................................................... 17 
Calcium silicate biomaterials ........................................................................ 19 
Calcium phosphate biomaterials ................................................................... 21 
Synthesis and characterization of calcium silicate and calcium
phosphate particles ........................................................................................ 23 
Sol-gel method to synthesize wollastonite particles ................................. 23 
Precipitation and hydrothermal methods to synthesize hydroxyapatite
with high aspect ratio ............................................................................... 24 
Precipitation method to synthesis nacreous like structures ...................... 26 
Cement preparation ....................................................................................... 29 
Setting time ................................................................................................... 30 
Static compressive strength and fatigue performance ................................... 31 
Quasi-static and compressive fatigue performance of four types
of dental restorations ................................................................................ 31 
Addition of calcium silicate materials on the compressive strength
of GIC ....................................................................................................... 33 
Addition of Ag-HA and Ag-DCPA on the compressive strength
of GIC ....................................................................................................... 34 
Bioactivity ..................................................................................................... 36 
Antibacterial properties ................................................................................. 41 
Cytotoxicity .................................................................................................. 44 
Conclusions ................................................................................................... 47 
Future perspectives ....................................................................................... 49
Analytical techniques and methods............................................................... 50 
X-ray diffraction ....................................................................................... 50 
SEM .......................................................................................................... 50 
Static compressive strength ...................................................................... 51 
Staircase method ...................................................................................... 51 
Antibacterial study ................................................................................... 52 
The Gilmore needle method ..................................................................... 52 
ICP-AES ................................................................................................... 53 
Sammanfatting på svenska ............................................................................ 54 
Acknowledgements ....................................................................................... 56 
References ..................................................................................................... 58